CN1882659A - Curable composition and elastic roller therefrom - Google Patents
Curable composition and elastic roller therefrom Download PDFInfo
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- CN1882659A CN1882659A CN 200480034499 CN200480034499A CN1882659A CN 1882659 A CN1882659 A CN 1882659A CN 200480034499 CN200480034499 CN 200480034499 CN 200480034499 A CN200480034499 A CN 200480034499A CN 1882659 A CN1882659 A CN 1882659A
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Abstract
Rollers assembled in an electrophotographic image forming apparatus have posed such a problem that when an elastic roller comprising a conductive shaft having at least one elastic layer disposed thereround and at least one coating layer disposed round the circumference thereof is rotated in contact with another member, detachment occurs at the interface of the elastic layer and the coating layer. This problem is solved by the use of a curable composition comprising as indispensable components (A) organic polymer having in its molecule at least one alkenyl capable of hydrosilylation reaction and having no alkoxy and/or epoxy, (B) compound having in its molecule at least two hydrosilyls, (C) hydrosilylation catalyst and (D) compound with the structure of the general formula: M-OR (1) (M: an atom selected from among silicon, aluminum and titanium atoms, and R: an organic group, such as alkyl or alkenyl) and/or compound having an epoxy.
Description
Technical field
The present invention relates to that solidification compound solidifies the elastomerics obtain and the binding property of other materials is the solidification compound of purpose to give, or relate to the electrophotographic copier of packing into, laser beam printer, facsimile recorder, utilize the technical field of the solidification compound of the resilient roller in these the image processing system of electrofax mode of compound business automation equipment etc.
Background technology
Roller in the aforementioned technical field uses by the purposes of charged roller, developing roll and fixing roller etc., at the desired characteristic difference of various uses.These rollers require characteristic to establish a plurality of resin layers around conductive shaft according to it.For example, the roll-gap width in order to obtain to contact with miscellaneous part is established the elastic layer of soft.At the skin of this elastic layer, establish and suppress the contained low molecular composition of elastic layer, or suppress the coating that is applicable to various uses of the binding property etc. on roller surface to the oozing out of roller surface.Therefore, have various characteristic, proposed to meet the roller of various purposes, and established the multiwalled roller, become extremely important in the binding property at the interface of each layer by making each layer.Why? this is because the occasion that this roller not only contacts but also is rotated with miscellaneous part produces with the roller surface and contacts the friction that causes, and in bonding weak bed interface the cause that coating is peeled off takes place.
In recent years, business automation equipments such as the printer of electrofax mode or duplicating machine carry out high speed promptly, therefore require to improve the mandrel of the roller that is contained in business automation equipment inside and the binding property at the interface of elastic layer, elastic layer and coating etc.The high speed of business automation equipment, promptly per 1 minute printing number increases, and this illustrates that also the per 1 minute rotation number of roller increases, thus the stress that the roller surface need be stronger than the past, owing to peel off with the generation of insufficient adherent bed interface, so it is not good to produce image.In order to address this problem, as the fusible method that improves mandrel and elastic layer, proposed in elastic layer, to add the method (spy opens flat 11-231706) of the silicoorganic compound that contain epoxy group(ing), in addition, as improving the fusible method of elastic layer, proposed after establishing coupling agent on the elastic layer, the method (spy opens flat 9-292767) of formation coating with coating.Though proposed to improve in this wise the fusible technology of elastic layer and coating, in the development of business automation equipment high speed, expectation improves binding property more than method in the past.
Summary of the invention
The present invention finishes in view of described actual state, its objective is provide improve to adopt conductive shaft around the solidification compound of peeling off of the bed interface that taken place when rotating of the roller that uses of the electrofax mode that constitutes of at least 1 layer coating forming of at least 1 layer elastic layer and this elastic layer periphery with miscellaneous part limit contact edge reach resilient roller by said composition system.
The inventor is in order to solve aforementioned problems, the discovery of concentrating on studies repeatedly, contain the alkenyl that at least 1 energy hydrogenation silylation reactive is arranged in (A) molecule by use, and be not selected from the organic polymer of at least 1 above group of alkoxyl group, epoxy group(ing), (B) compound of at least 2 hydrogenation silyls is arranged in the molecule, (C) hydrogenation silylanizing catalyzer (D) contains and is selected from following general formula (1)
M-OR (1)
(M is the atom that is selected from Siliciumatom, aluminium atom, titanium atom, and R is an alkyl)
Shown in the solidification compound of the compound of structure more than at least a kind of structure, epoxy group(ing) structure, the binding property of this solidification compound elastic layer that constitutes and the coating that is located at its periphery is improved, can suppress the peeling off of interface of elastic layer and coating, thereby finish the present invention.
In a kind of embodiment, preferably making aforementioned (A) composition and (D) mixing ratio by weight of composition is 90.0: 10.0～99.7: 0.3 scope.
In a kind of embodiment, the alkenyl of at least 1 energy hydrogenation silylation reactive is arranged in preferably aforementioned (D) component molecules.
In a kind of embodiment, 3 substituting groups on the contained two keys of the alkenyl of preferably aforementioned (D) composition are made of hydrogen.
In a kind of embodiment, preferably make aforementioned (B) composition have (D) composition of the alkenyl of at least 1 energy hydrogenation silylation reactive to react in advance with in the molecule, synthetic (E) composition.
In a kind of embodiment, in the polymkeric substance of preferred (A) composition, contain the alkenyl of energy hydrogenation silylation reactive in molecular end.
In a kind of embodiment, the organic polymer of preferably aforementioned (A) composition is the olefin oxide based polymer.
In a kind of embodiment, preferably in aforementioned solidification compound, add (F) electroconductibility imparting agent.
In a kind of embodiment, the ASKER-C hardness that preferred aforementioned solidification compound solidifies the rubber elastomer that obtains is 20～80 ° scope.
In a kind of embodiment, preferably around conductive shaft, establish the elastic layer of at least 1 layer aforementioned solidification compound formation.
In a kind of embodiment, preferably on the periphery of aforementioned elastic layer, establish at least 1 layer coating.
In a kind of embodiment, preferred aforementioned coating is made of the compound that urethane bond is arranged.
In a kind of embodiment, after preferably aforementioned elastic layer surface being carried out primary coat and handled, form coating.
The preferred plan that carries out an invention
Below, embodiment of the present invention are at length described.
(A) of the present invention composition, the alkenyl of at least 1 energy hydrogenation silylation reactive is arranged in the so-called molecule and is not selected from the organic polymer of group more than at least a kind of alkoxyl group, epoxy group(ing), as necessary functional group, at least 1 alkenyl is arranged, do not have any group at least in alkoxyl group and the epoxy group(ing), two kinds of groups all do not have sometimes.As other functional group, can there be particular restriction from selecting the functional group arbitrarily.
The alkenyl of so-called (A) composition so long as contain group to the two keys of the activated C=C of hydrogenation silylation reactive, does not then have particular restriction.As alkenyl, can enumerate the unsaturated aliphatic hydrocarbon base of vinyl, allyl group, methyl ethylene, propenyl, butenyl, pentenyl, hexenyl etc., the ring type unsaturated alkyl of cyclopropenyl radical, cyclobutene base, cyclopentenyl, cyclohexenyl etc., isobutenyl etc.Suitable is that it is good to be conceived to solidified nature, the preferred especially alkenyl that uses following general formula (2) expression.
H
2C＝C(R
1)-CH
2- (2)
(in the formula, R
1Be hydrogen atom or methyl)
In addition, with regard to (A) composition, be preferably in the alkenyl that polymer ends imports above-mentioned energy hydrogenation silylation reactive.When alkenyl was in polymer ends like this, the viewpoint that increases, obtains easily high-intensity rubber-like cured article etc. from the effective network chain amount of the cured article of final formation was considered and preferred.
In addition, (A) main chain of composition can not have particular restriction from selecting the polymkeric substance arbitrarily.For example, can enumerate polyisoprene, polyhutadiene, polyisobutene, sovprene, polyoxygenated alkene, polysiloxane, polythioether, urethane, polyacrylic ester etc.These polymkeric substance can use separately, also can and usefulness, can also make multipolymer and use.The polymkeric substance that constitutes of olefin oxide unit particularly is before the curing, owing to be low viscosity, operation easily, and the occasion of using aspect the purposes of resilient roller are because cured article has the structure of particularly soft, even it is thin its elastic effect of also giving full play to of wall, thereby preferred.
In addition, the so-called aforementioned olefin oxide based polymer that uses as (A) composition of solidification compound of the present invention is meant in the unit that constitutes main chain more than 30%, the preferred polymkeric substance that is made of the olefin oxide unit more than 50%, as the unit that is contained beyond the olefin oxide unit, can enumerate that initiator when making polymkeric substance uses, 2 above compound bearing active hydrogen, for example deutero-unit such as ethylene glycol, bis-phenol based compound, glycerol, TriMethylolPropane(TMP), tetramethylolmethane are arranged.In addition, it is a kind of that the olefin oxide unit there is no need, and also can be the multipolymer (also containing graftomer) of formations such as oxyethane, propylene oxide, butylene oxide ring.Aspect the environmental stability of electrical characteristic, as main chain backbone, preferably contain the lower propylene oxide unit of water-absorbent, or the unitary polymkeric substance of oxybutylene, if be considered to this aspect, especially preferably contain the polymkeric substance of propylene oxide unit.
As the molecular weight of such polyoxygenated olefin polymer, the viewpoint of the caoutchouc elasticity from its easily operation, after solidifying considers that preferred number average molecular weight (GPC method, polystyrene conversion) is 500～50,000.Number-average molecular weight is lower than 500 occasion, when being solidified, this solidification compound is difficult to obtain sufficient mechanical characteristics (rubber hardness, and number-average molecular weight is the occasion more than 50,000 elongation) etc.,, because the molecular weight of contained per 1 alkenyl increases in the molecule, or because of sterically hindered and reactive reduction, so often solidify insufficient, in addition, viscosity is too high, also has the tendency of processibility variation.
Secondly, solidifying agent as aforementioned (B) composition, it can be the compound that at least 2 hydrogenation silyls are arranged in the molecule, but when the number of the hydrogenation silyl that contains in the molecule is too many, remain in easily in the cured article owing to solidify a large amount of hydrogenation silyl in back, become the reason of cavity or be full of cracks, so preferred number with the hydrogenation silyl is adjusted to below 50, from the caoutchouc elasticity of control cured article or the good viewpoint of package stability is considered, more preferably be adjusted to 2～30.Moreover among the present invention, what is called has 1 hydrogenation silyl, and meaning has 1 and Si bonded H.Therefore, SiH
2Occasion, becoming has 2 hydrogenation silyls, but considers from the viewpoint of solidified nature and caoutchouc elasticity, preferably is combined on the different Si with Si bonded H.
The molecular weight of such solidifying agent considers that from the good viewpoint of processibility that makes the moulding product preferred number average molecular weight (Mn) is adjusted to below 30,000.In addition, consider that more preferably Mn is adjusted at 300～10,000 from making with the good viewpoint of the reactivity of above-mentioned base polymer or consistency.
In addition, above solidifying agent, if consider that the cohesive force of base polymer is bigger than the cohesive force of solidifying agent, be conceived to consistency, the modification body that contains phenyl is then importantly arranged, be conceived to obtain easily, then optimization styrene modification body, consider that from the viewpoint of package stability suitable is alpha-methyl styrene modification body.
Hydrogenation silylanizing catalyzer to as (C) composition does not have particular restriction, can use the catalyzer of hydrogenation silylanizing arbitrarily.If illustrate particularly, can enumerate Platinic chloride, platinum simple substance, the catalyzer of supported solid platinum on the carrier of aluminum oxide, silicon oxide, carbon black etc.; Platinum-vinylsiloxane complex compound { for example, Pt
n(ViMe
2SiOSiMe
2Vi)
m, Pt[(MeViSiO)
4]
m; Platinum-phosphine complex compound { for example, Pt (PPh
3)
4, Pt (PBu
3)
4; Platinum-phosphite complex compound { for example, Pt[P (OPh)
3]
4, Pt (P (OBu)
3)
4(in the formula, Me represents methyl, and Bu represents butyl, and Vi represents vinyl, and Ph represents phenyl, and n, m represent integer), Pt (acac)
2, also have Ashby etc. at the platinum-hydrocarbon complex body described in United States Patent (USP) the 3159601st and No. 3159662 specification sheetss, and Lamoreaux etc. is at the platinum-alcoholate catalyst described in No. 3220972 specification sheets of United States Patent (USP).
As the example of the catalyzer beyond the platinic compound, can enumerate RhCl (PPh
3)
3, RhCl
3, Rh/Al
2O
3, RuCl
3, IrCl
3, FeCl
3, AlCl
3, PdCl
22H
2O, NiCl
2, TiCl
4Deng.These catalyzer may be used alone, two or more kinds can also be used.Consider preferred Platinic chloride, platinum-alkene complex, platinum-vinylsiloxane complex compound, Pt (acac) from the viewpoint of catalytic activity
2Deng.As catalytic amount, there is not particular restriction, but with respect to 1 mole of the alkenyl in (A) composition, can be 10
-1～10
-8The scope of mole is used.To carry out the hydrogenation silylation reactive fully, more preferably 10
-2～10
-6The scope of mole is used.In addition, hydrogenation silylanizing catalyzer is generally very expensive and be corrodibility, and produces hydrogen in a large number, and cured article foaming sometimes is not so use 10
-1The above amount of mole is for well.
Below, (D) composition is described.
What is called contains the compound of structure more than at least a kind that is selected from structure, epoxy group(ing) structure shown in the following general formula (1),
M-OR (1)
(in the formula, M is selected from Siliciumatom, the aluminium atom, the atom of titanium atom, R are alkyl) and be the compound that contains at least a structure of aforementioned M-OR and epoxy group(ing) in the molecule, also can be the compound that contains M-OR and these two kinds of structures of epoxy group(ing).
The structure of so-called following general formula (1) expression
M-OR (1)
(in the formula, M is selected from Siliciumatom, the aluminium atom, the atom of titanium atom, R are alkyl) so long as contain in the molecule and be selected from Siliciumatom, the aluminium atom, at least a kind of atom of titanium atom (M that is equivalent to general formula (1)), and on this atom in conjunction with the compound of alkoxyl group, then do not have particular determination.As the alkyl (R that is equivalent to general formula (1)) of the alkyl that forms alkoxyl group etc., can enumerate methyl, ethyl, n-propyl, sec.-propyl, normal-butyl, sec-butyl, isobutyl-, the tertiary butyl, n-hexyl, n-octyl, cyclohexyl, phenyl, tolyl etc.As the concrete example of this compound, can enumerate commercially available silane coupling agent, titanium coupling agent, aluminum coupling agent.
In addition, (D) compound that contains epoxy group(ing) of composition is so long as have
(R
1～R
4Be organic radical or hydrogen atom arbitrarily) functional group of structure, then there is not particular restriction, particularly, can enumerate glycidyl, ester ring type epoxy group(ing), the epoxy group(ing) of aliphatic epoxy base etc.Because along with the number of the epoxy group(ing) of per 1 molecule increases, the package stability variation as (D) composition of the compound that contains epoxy group(ing) so contain 1～4 epoxy group(ing) in preferred 1 molecule, preferably contains 1～2 epoxy group(ing) again.
The mixing ratio by weight of aforementioned (A) composition and (D) composition preferably 90.0: 10.0～99.7: 0.3, and 95.0: 5.0～99.5: 0.5 occasion, can bring into play the excellent resilience restoring force of the elastic layer that (A)～(C) composition constitutes for solidification compound that must composition by the square and make the feature of two aspects of the binding property raising of elastic layer and coating because of adding (D) composition.The occasion of addition below 0.3 weight part of aforementioned (D) composition, because the binding property between elastic layer and coating is insufficient and undesirable, otherwise the above occasion of 10.0 weight parts is undesirable because compression set increases.
In order further to improve the binding property of elastic layer and coating, preferably (D) composition contains and is selected from following general formula (1)
M-OR (1)
(in the formula, M is selected from Siliciumatom, the aluminium atom, the atom of titanium atom, R are alkyl)
Shown in the structure more than at least a kind of structure, epoxy group(ing) structure, and contain the alkenyl of at least 1 energy hydrogenation silylation reactive in the molecule.This estimation is because of alkenyl of (D) composition and (B) the hydrogenation silyl reaction of composition, thus and the cause of alkoxyl group and/or epoxy group(ing) and coating reaction or the raising of interaction bounding force.
The alkenyl of so-called (D) composition so long as contain group to the two keys of the activated C=C of hydrogenation silylation reactive, does not then have particular restriction.As alkenyl, can enumerate vinyl, allyl group, methyl ethylene, propenyl, butenyl, pentenyl, the unsaturated aliphatic hydrocarbon base of hexenyl etc., cyclopropenyl radical, cyclobutene base, cyclopentenyl, the ring type unsaturated alkyl of cyclohexenyl etc., isobutenyl etc.With (B) composition nonreactive fully (D) composition, from the elastomerics that this solidification compound makes, ooze out, might pollute miscellaneous part; And, owing to do not combine with the hydrogenation silyl chemistry of (B) composition, so also poor with the binding property of coating.When on the alkenyl of hydrogenation silylation reactive substituting group being arranged, the hydrogenation silylation reactive is slack-off, and (D) composition with (B) composition reaction does not increase, so 3 substituting groups on the contained two keys of special preference chain thiazolinyl are made of hydrogen.For example, can enumerate vinyl, allyl group etc.
(E) composition is to make (D) composition of the alkenyl that at least 1 energy hydrogenation silylation reactive is arranged in (B) composition and the molecule react the compound that obtains in advance, and in order to react, as catalyzer, (C) the hydrogenation silylanizing catalyzer of composition is necessary.Therefore, consider that preferred synthetic (B) composition and (D) (E) composition of composition reaction of making in advance removed unreacted (D) composition in postprocessing working procedures from can suppress the viewpoint that unreacted (D) composition oozes out from elastomerics.In addition because synthetic (E) composition must be again and (A) composition and (C) composition reaction, so on cooperating liquid state preferably.In order to obtain such proterties,,, has only 1 alkenyl in the preferred especially molecule in order not form crosslinking structure with (B) composition as (D) composition of (E) composition raw material.In addition, use the occasion of (E) composition as solidification compound, preferably adjusting (B) composition and (D) use level of composition, make and contain at least 2 hydrogenation silyls, perhaps, have the viewpoint of sufficient elasticity to consider from the resilient roller that can make solidification compound system, preferably by (E), (A) and (C) composition be to add (B) composition adjusting use level again in the solidification compound of composition.
Be contained in the roller in the business automation equipments such as printer or duplicating machine, because necessary controlling resistance in electroconductibility～semi-conductivity field, so preferably (A)～(D) composition be must composition solidification compound, or (A), (C) and (E) composition be must the solidification compound of composition in the electroconductibility imparting agent of interpolation conduct (F) composition again.As the electroconductibility imparting agent of (F) composition, can enumerate carbon black or metal oxide, the metal fine powder end, also can enumerate quaternary ammonium salt, the carboxylic acid group is arranged, sulfonic group, sulfate group, the organic compound of phosphate-based grade or polymkeric substance, ether-ether imide, or ether imide polymer, oxyethane-epihalohydrin multipolymer, the compound that conductive means may is arranged of representatives such as methoxy poly (ethylene glycol) acrylate, or the compound that is called static inhibitor of macromolecular compound etc. etc.(F) composition among the present invention can use separately, also can will also use more than 2 kinds.As above-mentioned sooty example, can enumerate furnace black, acetylene black, dim, thermally oxidized black, thermal black is glossy black etc.These sooty kinds, particle diameter etc. without limits.
(F) addition of composition is adjusted interpolation according to desirable conductive characteristic, and polymkeric substance 100 weight parts with respect to (A) composition preferably use 0.01～100 weight part, preferably use 0.1～50 weight part again.Addition is very little the time, and it is insufficient that the conduction that is presented is given ability, and addition is when too many, and the rising of the viscosity of solidification compound is big, and is might operation poor.In addition, because the kind or the addition difference of used electroconductibility imparting agent influence the hydrogenation silylation reactive, give the influence of material to the hydrogenation silylation reactive so preferably consider electroconductibility.
Among the present invention, as required, can suit to add various weighting agents, various function endowing agent, oxidation inhibitor, UV light absorber, pigment, tensio-active agent, solvent.As the object lesson of aforementioned weighting agent, can enumerate fine silica powder, metal fine powder, lime carbonate, clay, talcum, titanium oxide, zinc white, diatomite, barium sulfate etc.
In the solidification compound of the present invention,, can use the improved storage stability agent in order to improve package stability.As this improved storage stability agent, be the common stablizer of knowing as the preserving stabilizer of (B) of the present invention composition, so long as reach the compound of desired purpose, then there is not particular determination.Particularly, can suitably use the compound that contains the aliphatics unsaturated link(age), organo phosphorous compounds, organosulfur compound, nitrogenous compound, tin based compound, organo-peroxide etc.Again particularly, can enumerate 2-[4-morpholinodithio base sulfide, benzothiazole, thiazole, dimethyl acetylenedicarbexylate, acetylenedicarboxylic acid diethyl ester, butylhydroxy toluene, butyl hydroxyanisole, vitamin-E, 2-(4-morpholinodithio) benzothiazole, 3-methyl-1-butene-3-alcohol, the organo-siloxane that contains the acetylene series unsaturated group, the organo-siloxane that contains the olefinic unsaturated group, acetylene alcohol, 3-methyl isophthalic acid-butyl-3-alcohol, 3-methyl-pentyne-3-alcohol, diallyl fumarate, diallyl maleate, DEF, ethyl maleate, dimethyl maleate, the 2-pentenenitrile, 2,3-dichloropropylene etc., but be not limited to these.
In addition, the occasion of in the roller purposes of utilization of packing into, using as the image processing system of electrofax mode of the present invention, by preferably 20～80 ° of the ASKER-C hardness of the cured article of aforementioned solidification compound system, the occasion that the developing roll that particularly limit contacts with miscellaneous part, toning agent is carried on the limit uses, preferably 30～70 °.In the low field of hardness ratio aforementioned range, because hardness is too low, thus the compression set increase, on the contrary in the field of high rigidity,, toning agent is applied big stress because hardness is too high, thereby undesirable.
The resilient roller of solidification compound system of the present invention, use by the elastic layer that around conductive shaft, forms at least 1 layer aforementioned solidification compound formation, the formation method of the elastic layer of rubber rollers does not have particular determination, can use the forming method of known various rollers in the past.For example, be provided with in the mould of conductive shaft of SUS system etc. at the center, adopt extrusion moulding, extrusion forming, injection molding, reaction injection moulding (RIM), liquid injection molding (LIM), the various methods of forming of cast molding etc. are with composition molding, adopt suitable temperature and time to be heating and curing, around conductive shaft, form conductive elastic layer.Here, as the manufacture method of the conductive roll among the present invention, the solidification compound of using when the formation elastic layer is liquid occasion, considers preferred aqueous injection molding from the viewpoint of production efficiency, processibility.This occasion, solidification compound also can be provided with the technology of after fixing, completely solidified in addition behind semicure.
Aforementioned elastic layer is owing to often giving tackiness to the surface, so preferably establish the coating of one deck at least on the periphery of elastic layer.This coating preferably uses the few coating of tackiness.
Material as coating does not have particular restriction, but the occasion that the roller that limit and miscellaneous part contact edge are rotated uses, because wear resistance must be arranged, so the good compound that urethane bond is arranged of wear resistance preferably.In addition, coating must have the flexibility of appropriateness, consider from this viewpoint, preferably constitute for the polyurethane resin composition of mainly forming by resin with polyethers, polyester, polycarbonate skeleton, these compositions also can be the blending resins of polyether(poly)urethane, PAUR, polycarbonate polyurethane, or the polyurethane resin composition of amino-formate bond and at least a kind of skeleton selecting from polyethers, polyester, polycarbonate, polysiloxane is arranged in 1 molecule.
In addition, constitute the resin combination of upper layer,, adjust surface shape or the viewpoint of the binding property of conductive elastic layer etc. is considered, also can add the electroconductibility imparting agent as required, the various additives of various weighting agents etc. from regulating resistance.In order further to improve the elastic layer and the binding property of coating that solidification compound of the present invention constitutes, after preferably the elastic layer surface being carried out primary coat and handled, the formation coating.Silane coupling agent of the present invention can use various coupling agents or contain the silane coupling agent arbitrarily of epoxy compounds.
Formation method as coating of the present invention, there is not particular restriction, can be by on the periphery of the elastic layer that forms around the conductive shaft, adopt spraying, dip-coating, the resin combination of the method handle formation coating of roller coat etc. is coated with into the thickness of regulation, carries out drying under the temperature of regulation, solidify, form coating.Particularly, the resin dissolves of using as aforementioned coating in solvent and make solids component be 5～20% spray or the method for dip-coating very easy.As the solvent that uses, as long as and mix as the resin of the main component of the coating that uses, then do not have particular restriction, particularly, can enumerate methyl ethyl ketone, N-BUTYL ACETATE, vinyl acetic monomer, N, dinethylformamide, toluene, Virahol, water etc.Particularly use urethane resin to form the occasion of coating, consider preferred N, dinethylformamide, N,N-dimethylacetamide from the viewpoint of intermiscibility.Here, as the drying temperature of coating, preferred 70～200 ℃.When drying temperature is lower than 70 ℃, dry sometimes insufficient, during greater than 200 ℃, cause the elastic layer of internal layer aging sometimes.In addition, the thickness of coating is set suitable value for according to used material, composition and purposes etc., though there is not particular determination, common preferred 1～100 μ m, when thinner than 1 μ m, wear resistance reduces, the tendency that has long durability to reduce.In addition, when thicker, have to result from and wrinkle take place easily, or the tendency of the problem of compression set increase etc. takes place with the difference of the linear expansivity of elastic layer than 100 μ m.In order to adjust the thickness of coating, also can be with spraying method, methods such as dip coating repeat several times, repeat coating.Among the present invention,, also can add the various additives of flow agent etc. as required in order to improve the film-forming properties of coating solution.
Embodiment
Below, infinite embodiment of the present invention is described.
(embodiment 1)
Using three-roll mill 500g allyl capped polyoxypropylene (trade(brand)name ACX004-N, clock deep pool chemical industry system; Be equivalent to the A composition), 70g carbon black #3030B (Mitsubishi Chemical's system; Be equivalent to the F composition) in the mixing mixture, mix poly-organohydrogensiloxanes (trade(brand)name CR100, clock deep pool chemical industry system more equably; Be equivalent to the B composition) 16g, two (1,3-divinyl-1,1,3,3-tetramethyl disiloxane) platinum complex catalyst (platinum content 3 weight %, xylene solution; Be equivalent to the C composition) 350 μ L, dimethyl maleate 170 μ L, tetraethoxysilane (being equivalent to the D composition) 5g.Use vacuum defoamation whipping appts (シ one テ Star Network corporate system) that this solidification compound is carried out deaeration in 90 minutes.This solidification compound is expelled to mould (internal diameter 16mm) internal configuration to be had in this mould of SUS system axle of diameter 8mm, mould is left standstill to make it in 20 minutes to solidify under 140 ℃ environment.The ASKER-C hardness of the elastic layer roller that makes like this is shown in table 1.Then, by in using the ball mill mixture that 150g methylethylketone and 12g carbon black #3030B (Mitsubishi Chemical's system) is mixing, again polyurethane resin solution (trade(brand)name Ha イ system レ Application Y-258, the big day system of refining) furnishing 100g, N, dinethylformamide furnishing 300g makes the coating coating fluid.Adopt pickling process to be coated with aforementioned coating fluid, 140 ℃ of dryings 5 minutes.Repeat 1 same coating operation, dry under 160 ℃, 90 minutes condition in addition, coating is set.The roller that makes like this is fixed in the colour printer box (EP-85, Canon's system), this is box-packedly gone in the color printer (LASER SHOTLBP-2510, Canon's system), the peeling off of roller elastic layer behind 10000 images of visual observation output and coating.Be shown in table 1 peeling off observations.
(embodiment 2)
Using three-roll mill with 500g allyl capped polyoxypropylene (trade(brand)name ACX004-N, clock deep pool chemical industry system; Be equivalent to the A composition), with 70g#3030B (Mitsubishi Chemical's system; Be equivalent to the F composition) in the mixing mixture, mix the poly-organohydrogensiloxanes of 16g (trade(brand)name CR100, clock deep pool chemical industry system more equably; Be equivalent to the B composition), two (1,3-divinyl-1,1,3,3-tetramethyl disiloxane) platinum complex catalyst (platinum content 3 weight %, xylene solutions of 350 μ L; Be equivalent to the C composition), the dimethyl maleate of 170 μ L, the acetyl alkoxyl group di-isopropyl of 5g close aluminium (acetoalkoxyaluminumdiisopropylate, trade(brand)name AL-M, Ajinomoto Fine-Techno.Co.Inc. system; Be equivalent to the D composition).The elastic layer after ASKER-C hardness, the roller coating of the elastic layer roller that the method that adopts is similarly to Example 1 made forms and the stripping test result of coating are summarized in table 1.
(embodiment 3)
Using three-roll mill with 500g allyl capped polyoxypropylene (trade(brand)name ACX004-N, clock deep pool chemical industry system; Be equivalent to the A composition), 70g#3030B (Mitsubishi Chemical's system; Be equivalent to the F composition) in the mixing mixture, mix the poly-organohydrogensiloxanes of 16g (trade(brand)name CR100, clock deep pool chemical industry system more equably; Be equivalent to the B composition), two (1,3-divinyl-1,1,3,3-tetramethyl disiloxane) platinum complex catalyst (platinum content 3 weight %, xylene solutions of 350 μ L; Be equivalent to the C composition), four titanium butoxide of the dimethyl maleate of 170 μ L, 5g (being equivalent to the D composition).The elastic layer after ASKER-C hardness, the roller coating of the elastic layer roller that the method that adopts is similarly to Example 1 made forms and the stripping test result of coating are summarized in table 1.
(embodiment 4)
Using three-roll mill the allyl capped polyoxypropylene of 495g (trade(brand)name ACX004-N, clock deep pool chemical industry system; Be equivalent to the A composition), the #3030B of 70g (Mitsubishi Chemical's system; Be equivalent to the F composition) in the mixing mixture, poly-organohydrogensiloxanes (trade(brand)name CR100, the clock deep pool chemical industry system of mixing 19g more equably; Be equivalent to the B composition), two (1,3-divinyl-1,1,3,3-tetramethyl disiloxane) platinum complex catalyst (platinum content 3 weight %, xylene solutions of 430 μ L; Be equivalent to the C composition), the dimethyl maleate of 210 μ L, the trimethoxy vinyl silanes of 5g (being equivalent to the D composition).The elastic layer after ASKER-C hardness, the roller coating of the elastic layer roller that the method that adopts is similarly to Example 1 made forms and the stripping test result of coating are summarized in table 1.
(embodiment 5)
The poly-organohydrogensiloxanes of 16g (trade(brand)name CR100, clock deep pool chemical industry system; Be equivalent to the B composition) be heated to 100 ℃ with the synthetic solution of 30g toluene (following is a liquid), in a liquid that stirs, drip 5g trimethoxy vinyl silanes (being equivalent to the D composition), two (1 of 150 μ L, 3-divinyl-1,1,3, the 3-tetramethyl disiloxane) platinum complex catalyst (platinum content 3 weight %, xylene solution; Be equivalent to the C composition), the synthetic solution of 10g toluene.Stir after 5 hours, toluene and unreacted trimethoxy vinyl silanes are heated up in a steamer in decompression, make (E) composition.Then, in the allyl capped polyoxypropylene that uses three-roll mill with 495g (trade(brand)name ACX004-N, clock deep pool chemical industry system; Be equivalent to the A composition), 70g carbon black #3030B (Mitsubishi Chemical's system; Be equivalent to the F composition) in the mixing mixture, mix aforementioned (E) composition more equably, two (1,3-divinyl-1,1,3,3-tetramethyl disiloxane) platinum complex catalyst (platinum content 3 weight %, xylene solutions of 280 μ L; Be equivalent to the C composition), the dimethyl maleate of 140 μ L.The elastic layer after ASKER-C hardness, the roller coating of the elastic layer roller that the method that adopts is similarly to Example 1 made forms and the stripping test result of coating are summarized in table 1.
(embodiment 6)
Evenly be coated with on the elastic layer roller surface that the solidification compound that uses similarly to Example 1 makes by 2g A-187 (the outstanding Buddhist nun's blocking of Japan) with hairbrush, the synthetic primary coat solution of 2g four titanium butoxide and 100g methylethylketone, at 100 ℃, dry under 3 minutes the condition.Elastic layer roller employing method similarly to Example 1 to such primary coat is handled forms coating by dip coated, and the stripping test result of elastic layer and coating is summarized in table 1.
(embodiment 7)
Be coated with A-187 (the outstanding Buddhist nun's blocking of Japan) equably on the elastic layer roller surface that the solidification compound that uses similarly to Example 4 makes with hairbrush by 2g, four titanium butoxide of 2g, and the synthetic primary coat solution of 100g methylethylketone, at 100 ℃, dry under 3 minutes the condition.Elastic layer roller employing method similarly to Example 1 to such primary coat is handled forms coating by carrying out dip coated, and the stripping test result of elastic layer and coating is summarized in table 1.
(embodiment 8)
Using three-roll mill the allyl capped polyoxypropylene of 495g (trade(brand)name ACX004-N, clock deep pool chemical industry system; Be equivalent to the A composition), carbon black #3030B (Mitsubishi Chemical's system of 70g; Be equivalent to the F composition) in the mixing mixture, mix the poly-organohydrogensiloxanes of 21g (trade(brand)name CR100, clock deep pool chemical industry system more equably; Be equivalent to the B composition), two (1,3-divinyl-1,1,3,3-tetramethyl disiloxane) platinum complex catalyst (platinum content 3 weight %, xylene solutions of 480 μ L; Be equivalent to the C composition), the dimethyl maleate of 240 μ L, the glycidyl allyl ether of 5g (being equivalent to the D composition).The elastic layer after ASKER-C hardness, the roller coating of the elastic layer roller that the method that adopts is similarly to Example 1 made forms and the stripping test result of coating are summarized in table 1.
(embodiment 9)
Using three-roll mill the allyl capped polyoxypropylene of 495g (trade(brand)name ACX004-N, clock deep pool chemical industry system; Be equivalent to the A composition), the #3030B of 70g (Mitsubishi Chemical's system; Be equivalent to the F composition) in the mixing mixture, mix the poly-organohydrogensiloxanes of 21g (trade(brand)name CR100, clock deep pool chemical industry system more equably; Be equivalent to the B composition), two (1,3-divinyl-1,1,3,3-tetramethyl disiloxane) platinum complex catalyst (platinum content 3 weight %, xylene solutions of 480 μ L; Be equivalent to the C composition), the dimethyl maleate of 240 μ L, the 4 vinyl cyclohexene oxide compound of 5g (being equivalent to the D composition).The elastic layer after ASKER-C hardness, the roller coating of the elastic layer roller that the method that adopts is similarly to Example 1 made forms and the stripping test result of coating are summarized in table 1.
(embodiment 10)
The poly-organohydrogensiloxanes of 21g (trade(brand)name CR100, clock deep pool chemical industry system; Be equivalent to the B composition) be heated to 100 ℃ with the synthetic solution of 30g toluene (following is a liquid), Dropwise 5 g glycidyl allyl ether (being equivalent to the D composition) in a liquid that stirs, two (1 of 200 μ L, 3-divinyl-1,1,3, the 3-tetramethyl disiloxane) platinum complex catalyst (platinum content 3 weight %, xylene solution; Be equivalent to the C composition), the synthetic solution of 10g toluene stirred after 5 hours, and toluene and unreacted glycidyl allyl ether are heated up in a steamer in decompression, make (E) composition.Then, using three-roll mill the allyl capped polyoxypropylene of 495g (trade(brand)name ACX004-N, clock deep pool chemical industry system; Be equivalent to the A composition), 70g carbon black #3030B (Mitsubishi Chemical's system; Be equivalent to the F composition) in the mixing mixture, uniform mixing aforementioned (E) composition again, two (1,3-divinyl-1,1,3,3-tetramethyl disiloxane) platinum complex catalyst (platinum content 3 weight %, xylene solutions of 280 μ L; Be equivalent to the C composition), the dimethyl maleate of 240 μ L.The elastic layer after ASKER-C hardness, the roller coating of the elastic layer roller that the method that adopts is similarly to Example 1 made forms and the stripping test result of coating are summarized in table 1.
(embodiment 11)
With hairbrush on elastic layer roller surface that the solidification compound that uses similarly to Example 8 makes, be coated with A-187 (the outstanding Buddhist nun's blocking of Japan) equably by 2g, the synthetic primary coat solution of 2g four titanium butoxide and 100g methylethylketone, dry under 100 ℃, 3 minutes condition.Elastic layer roller employing method similarly to Example 1 to such primary coat is handled forms coating by carrying out dip coated, and the stripping test result of elastic layer and coating is summarized in table 1.
(comparative example 1)
Using three-roll mill the allyl capped polyoxypropylene of 500g (trade(brand)name ACX004-N, clock deep pool chemical industry system; Be equivalent to the A composition), the #3030B of 70g (Mitsubishi Chemical's system; Be equivalent to the F composition) in the mixing mixture, mix the poly-organohydrogensiloxanes of 16g (trade(brand)name CR100, clock deep pool chemical industry system more equably; Be equivalent to the B composition), two (1,3-divinyl-1,1,3,3-tetramethyl disiloxane) platinum complex catalyst (platinum content 3 weight %, xylene solutions of 350 μ L; Be equivalent to the C composition), the dimethyl maleate of 170 μ L.The elastic layer after ASKER-C hardness, the roller coating of the elastic layer roller that the method that adopts is similarly to Example 1 made forms and the stripping test result of coating are summarized in table 1.
Table 1
| Roller hardness (ASKER-C) | Peeling off of elastic layer and coating interface | |
| Embodiment 1 | 49 | ○△ |
| Embodiment 2 | 50 | ○△ |
| Embodiment 3 | 51 | ○△ |
| Embodiment 4 | 46 | ○ |
| Embodiment 5 | 48 | ○ |
| Embodiment 6 | Identical with embodiment 1 | ○ |
| Embodiment 7 | Identical with embodiment 4 | ◎ |
| Embodiment 8 | 43 | ○ |
| Embodiment 9 | 44 | ○ |
| Embodiment 10 | 45 | ○ |
| Embodiment 11 | Identical with embodiment 8 | ◎ |
| Comparative example 1 | 49 | × |
Peeling off of coating
◎: this test is not peeled off, and does not peel off fully with the hand stripping yet.
Zero: this test is not peeled off, and may peel off but force with the hand stripping.
Zero △: this test is not peeled off, but some wrinkle appear in coating.
*: occur peeling off.
The possibility of utilizing on the industry
Adopt solidification compound of the present invention and by the resilient roller of said composition system, generation peeled off when the roller limit that can suppress to be contained in the business automation equipment inside of the printer of electrofax mode or duplicator etc. was rotated with the miscellaneous part contact edge.
Claims (13)
1. with following (A)～(D) composition the solidification compound of necessary composition,
(A) alkenyl of at least 1 energy hydrogenation silylation reactive is arranged in the molecule, and is not selected from the organic polymer of group more than at least a kind of alkoxyl group, epoxy group(ing),
(B) compound of at least 2 hydrogenation silyls is arranged in the molecule,
(C) hydrogenation silylanizing catalyzer,
(D) contain at least and be selected from following general formula (1)
M-OR (1)
(M is the atom that is selected from Siliciumatom, aluminium atom, titanium atom, and R is an alkyl)
Shown in the compound of structure more than at least a kind of structure, epoxy group(ing) structure.
2. the described solidification compound of claim 1 is characterized in that, making aforementioned (A) composition and (D) the weight compounding ratio of composition is 90.0: 10.0～99.7: 0.3 scope.
3. the described solidification compound of any one of claim 1～2 is characterized in that, aforementioned (D) composition has the alkenyl of at least 1 energy hydrogenation silylation reactive in molecule.
4. the described solidification compound of claim 3 is characterized in that, three substituting groups on the contained two keys of the alkenyl of aforementioned (D) composition are made of hydrogen.
5. the described solidification compound of any one of claim 3～4, wherein, with (D) composition reaction synthetic (E) composition of alkenyl that at least 1 energy hydrogenation silylation reactive is arranged in aforementioned (B) composition by making and the molecule in advance, (A) composition and (C) composition be necessary composition.
6. the described solidification compound of any one of claim 1～5 wherein, (A) in the polymkeric substance of composition, contains the alkenyl of energy hydrogenation silylation reactive in molecular end.
7. the described solidification compound of any one of claim 1～6 is characterized in that, the organic polymer of aforementioned (A) composition is the olefin oxide based polymer.
8. the described solidification compound of any one of claim 1～7 is characterized in that, adds (F) electroconductibility imparting agent in any one described solidification compound of aforementioned claim 1～7.
9. the described solidification compound of any one of claim 1～8 is characterized in that, the elastomeric ASKER-C hardness that aforementioned solidification compound curing makes is 20～80 ° scope.
10. resilient roller is wherein established the elastic layer that any one described solidification compound of at least 1 layer claim 1～9 constitutes around conductive shaft.
11. the described resilient roller of claim 10 is characterized in that, establishes at least 1 layer coating on the periphery of aforementioned elastic layer.
12. the described resilient roller of claim 11 is characterized in that aforementioned coating is made of the compound with amino-formate bond.
13. the described resilient roller of any one of claim 11～12 is characterized in that, for any one described resilient roller of claim 11～12, after the elastic layer surface carried out primary coat and handle, forms coating.
Applications Claiming Priority (3)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP2003403852 | 2003-12-02 | ||
| JP403852/2003 | 2003-12-02 | ||
| JP431660/2003 | 2003-12-25 |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN1882659A true CN1882659A (en) | 2006-12-20 |
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ID=37520197
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN 200480034499 Pending CN1882659A (en) | 2003-12-02 | 2004-11-19 | Curable composition and elastic roller therefrom |
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| CN (1) | CN1882659A (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US8642148B2 (en) | 2008-08-22 | 2014-02-04 | Bridgestone Corporation | Electrifying roller |
| CN110955132A (en) * | 2018-09-26 | 2020-04-03 | 富士施乐株式会社 | Fixing member, fixing device, process cartridge, and image forming apparatus |
-
2004
- 2004-11-19 CN CN 200480034499 patent/CN1882659A/en active Pending
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US8642148B2 (en) | 2008-08-22 | 2014-02-04 | Bridgestone Corporation | Electrifying roller |
| CN102132221B (en) * | 2008-08-22 | 2016-04-06 | 株式会社普利司通 | Charged roller |
| CN110955132A (en) * | 2018-09-26 | 2020-04-03 | 富士施乐株式会社 | Fixing member, fixing device, process cartridge, and image forming apparatus |
| CN110955132B (en) * | 2018-09-26 | 2023-10-10 | 富士胶片商业创新有限公司 | Fixing member, fixing device, process cartridge, and image forming apparatus |
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